CN103469183A - Method for metallizing surface of alumina ceramic substrate - Google Patents
Method for metallizing surface of alumina ceramic substrate Download PDFInfo
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Abstract
The invention discloses a method for metallizing surface of an alumina ceramic substrate. The method comprises unit processes of coarsening pretreatment, primary nickel plating and secondary copper plating, wherein the coarsening pretreatment comprises: ultrasonically treating the alumina ceramic substrate in coarsening liquid for 20-40 min, and then, washing the alumina ceramic substrate through deionized water to obtain a pre-treated substrate; the primary nickel plating comprises: putting the pre-treated substrate in a plating solution I, ultrasonically depositing for 40-60 min at room temperature, washing the pre-treated substrate through deionized water after taking out the same, and drying the pre-treated substrate to obtain a nickel-plated substrate; the secondary copper plating comprises: putting the nickel-plated substrate in a plating solution II, reacting at 60-80 DEG C for 40-60 min, taking out the nickel-plated substrate after cooling the same, washing the nickel-plated substrate through deionized water, and drying the nickel-plated substrate to obtain a copper-plated substrate. A metal copper layer on the surface of the alumina ceramic substrate prepared by the method disclosed by the invention is good in combination with the substrate, good in coating density and uniform in structure components.
Description
One, technical field
The present invention relates to a kind of method of aluminium oxide ceramic substrate surface metalation, by the secondary electroless plating, complete the aluminium oxide ceramic substrate copper coating.
Two, background technology
The aluminium oxide ceramic substrate surface metalation can make pottery and metal couple together and make composite base plate, combines heat conduction, the conductivity of the good mechanical property of stupalith and metallic substance excellence, is the gordian technique of electrovacuum ceramics device production.Often run into following problem in the alumina-ceramic metallization processes: Metallization strength is on the low side, membranous layer binding force is poor, density is low, metallization face printing opacity, easily oxidation etc.These not only cause yield rate to lower, and affect quality product, and therefore constantly research improves the metallization process level, most important for the development of improving the quality of products, promote vacuum electron device.At present, the method for ceramic metallization mainly contains electroless plating method, electrochemical plating, high temperature sintering by Ag (Ni) method, Mo-Mn sintering process, vacuum evaporatation and vacuum sputtering coating method.Traditional Mn-Mo sintering process is owing to being high temperature sintering, and not only power consumption is large, and can not be applicable to the paster skeleton that high molecular polymer etc. is made.Although that electrochemical plating and ceramic junction are made a concerted effort is strong, internal stress is little, significantly shortcoming is that the metallized clean impact with the pure degree of plating solution on porcelain piece surface is large.Electroless plating is one of comparatively common method of ceramic metallization, but, because the aluminium oxide ceramic substrate surface does not possess catalytic activity, in industrial production, the catalytic activation that generally need to contain precious metal is processed, and still contains the elements such as precious metals pd, complex process.
Three, summary of the invention
The present invention aims to provide a kind of method of aluminium oxide ceramic substrate surface metalation, does not need sensitization and activation treatment, easy and simple to handle, can not produce heavy metal contamination, economizes on resources.The metal copper layer on the aluminium oxide ceramic substrate surface that the present invention is prepared, the film base is in conjunction with good, and coating compactness is good, and structural constituent is even.
The present invention is at first by the alligatoring pre-treatment, utilize coarsening solution to make ceramic base plate surface produce certain roughness to the corrasion on aluminum oxide substrate surface, then carrying out ultrasonic wave assistant chemical nickel plating for the first time processes, wherein the stability of chemical plating fluid is not high, thereby can make a certain amount of equally distributed nickel particle of aluminium oxide ceramic substrate surface deposition in the electroless plating process, pass through again electroless copper for the second time, the nickle atom that produces of take in electroless plating for the first time has certain thickness as reaction activation center forms alumina surface, uniformly copper plate.
Technical solution problem of the present invention adopts following technical scheme:
The method of aluminium oxide ceramic substrate surface metalation of the present invention comprises alligatoring pre-treatment, a nickel plating and each unit process of secondary copper facing:
Described alligatoring pre-treatment is that aluminium oxide ceramic substrate is placed in to coarsening solution supersound process 20-40 minute, adopts afterwards deionized water rinsing, obtains pretreated substrate;
The aqueous solution that described coarsening solution is hydrofluoric acid and Neutral ammonium fluoride, in described coarsening solution, the concentration of hydrofluoric acid is 20-60ml/L, the concentration of Neutral ammonium fluoride is 1-4g/L.
A described nickel plating is that described pretreated substrate is placed in to the plating solution I, and ultrasonic deposition 40-60 minute under room temperature uses deionized water rinsing after taking out, and, in 80-100 ℃ of oven drying 2-4 hour, obtains the nickel plating substrate;
Described plating solution I is the aqueous solution of single nickel salt, inferior sodium phosphate, boric acid and Trisodium Citrate, in described plating solution I, the concentration of single nickel salt is 20-30g/L, the ortho phosphorous acid na concn is 22-27g/L, and the concentration of boric acid is 24-30g/L, and the concentration of Trisodium Citrate is 50-60g/L.The pH value of described plating solution I is adjusted to 10-11 with sodium hydroxide.
Described secondary copper facing is that described nickel plating substrate is placed in to the plating solution II, turns one's coat to bathe in 60-80 ℃ and answers 40-60 minute, and cooling rear taking-up deionized water rinsing, obtain the copper facing substrate after drying.
Described plating solution II is copper sulfate, formaldehyde, disodium ethylene diamine tetraacetate and 2, the aqueous solution of 2-dipyridyl, in described plating solution II, the concentration of copper sulfate is 10-13g/L, 2, the concentration of 2-dipyridyl is 0.03-0.05g/L, the concentration of formaldehyde is 15-25mL/L, and the concentration of disodium ethylene diamine tetraacetate is 35-45g/L.The pH value of described plating solution II is adjusted to 11-12 with sodium hydroxide.
Ultrasonic frequency during described ultrasonic deposition is 40KHz, and power is 300-400W.
The present invention adopts pretreatment fluid to carry out alligatoring pre-treatment before electroless plating to aluminium oxide ceramic substrate, then by the auxiliary secondary chemical plating method of normal temperature ultrasonic wave at aluminium oxide ceramic substrate surface growth chemical plating copper layer.Whole process is easy, easy to operate, can not produce heavy metal contamination, and very large economic and social benefits are arranged.
Compared with the prior art, beneficial effect of the present invention is embodied in:
Chemical plating technology of the present invention does not need sensitization and activation treatment, by the alligatoring pre-treatment, in conjunction with the auxiliary secondary electroless plating of normal temperature ultrasonic wave, carries out the metallized technique of alumina surface, easy and simple to handle, can reduce pollution, economizes on resources.The aluminium oxide ceramic substrate surface metal copper layer that the present invention is prepared, the film base is in conjunction with good, and coating compactness is good, and structural constituent is even.
Below in conjunction with drawings and Examples, the present invention is described further, and it is more obvious that purpose of the present invention and effect will become.
Four, accompanying drawing explanation
Fig. 1 is the surface topography photo after aluminium oxide ceramic substrate process alligatoring pre-treatment in the embodiment of the present invention 1.As can be seen from Figure 1 alumina surface inclusion-free existence, grain edges, and particle surface has certain surface imperfection and depression.
Fig. 2 is the surface topography of nickel plating substrate in the embodiment of the present invention 1.As can be seen from Figure 2 the nickel plating substrate surface has deposited the nickel particle of many submicron orders, is evenly distributed in its surface.
Fig. 3 is the surface topography of copper facing substrate in the embodiment of the present invention 1.As can be seen from Figure 3 copper facing substrate surface metal tunic base is in conjunction with good, and coating compactness is good, and structural constituent is even.
Five, embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
1, alligatoring pre-treatment
In room temperature, air atmosphere, aluminium oxide ceramic substrate is placed in to coarsening solution, supersound process 30 minutes, adopt deionized water rinsing afterwards, obtains pretreated substrate.
The aqueous solution that described coarsening solution is hydrofluoric acid and Neutral ammonium fluoride, in coarsening solution, hydrofluoric acid concentration is 40ml/L, Neutral ammonium fluoride concentration 2g/L.
2, a nickel plating
To insert in the plating solution I through pretreated alumina-ceramic sample, after being 10 with sodium hydroxide adjusting pH, ultrasonic deposition 50 minutes, the ultrasonic frequency of ultrasonic deposition is 40KHz, and power is 300W, has reacted rear taking-up sample, use deionized water rinsing, and, in 90 ℃ of oven dryings 3 hours, room temperature is cooling, obtains the nickel plating substrate.
The aqueous solution that described plating solution I is single nickel salt, inferior sodium phosphate, boric acid and Trisodium Citrate, wherein the concentration of single nickel salt is 25g/L, and the ortho phosphorous acid na concn is 25g/L, and the concentration of boric acid is 25g/L, and the concentration of Trisodium Citrate is 55g/L.
3, secondary copper facing
The nickel plating substrate is put into to the plating solution II, and regulating pH with sodium hydroxide is 12,60 ℃ of heating in water bath for reaction 50 minutes, is cooled to room temperature with liquid afterwards, by deionized water rinsing drying, obtains the copper facing substrate.
The aqueous solution that described plating solution II is copper sulfate, formaldehyde, disodium ethylene diamine tetraacetate and 2,2-dipyridyl, wherein the concentration of copper sulfate is 12g/L, the concentration of formaldehyde is 20mL/L, the concentration of disodium ethylene diamine tetraacetate is 40g/L, and the concentration of 2,2-dipyridyl is 0.04g/L.
Alumina-ceramic surface metal copper layer prepared by the present embodiment, the film base is in conjunction with good, and coating compactness is good, and structural constituent is even.
Embodiment 2:
1, alligatoring pre-treatment
In room temperature, air atmosphere, aluminium oxide ceramic substrate is placed in to coarsening solution, supersound process 40 minutes, adopt deionized water rinsing afterwards, obtains pretreated substrate.
The aqueous solution that described coarsening solution is hydrofluoric acid and Neutral ammonium fluoride, in coarsening solution, hydrofluoric acid concentration is 60ml/L, Neutral ammonium fluoride concentration 4g/L.
2, a nickel plating
To insert in the plating solution I through pretreated alumina-ceramic sample, after being 11 with sodium hydroxide adjusting pH, ultrasonic deposition 40 minutes, the ultrasonic frequency of ultrasonic deposition is 40KHz, and power is 300W, has reacted rear taking-up sample, use deionized water rinsing, and, in 100 ℃ of oven dryings 4 hours, room temperature is cooling, obtains the nickel plating substrate.
The aqueous solution that described plating solution I is single nickel salt, inferior sodium phosphate, boric acid and Trisodium Citrate, wherein the concentration of single nickel salt is 20g/L, and the ortho phosphorous acid na concn is 22g/L, and the concentration of boric acid is 24g/L, and the concentration of Trisodium Citrate is 50g/L.
3, secondary copper facing
The nickel plating substrate is put into to the plating solution II, and regulating pH with sodium hydroxide is 11,70 ℃ of heating in water bath for reaction 50 minutes, is cooled to room temperature with liquid afterwards, by deionized water rinsing drying, obtains the copper facing substrate.
The aqueous solution that described plating solution II is copper sulfate, formaldehyde, disodium ethylene diamine tetraacetate and 2,2-dipyridyl, wherein the concentration of copper sulfate is 10g/L, the concentration of formaldehyde is 15mL/L, the concentration of disodium ethylene diamine tetraacetate is 35g/L, and the concentration of 2,2-dipyridyl is 0.03g/L.
Alumina-ceramic surface metal copper layer prepared by the present embodiment, the film base is in conjunction with good, and coating compactness is good, and structural constituent is even.
Embodiment 3:
1, alligatoring pre-treatment
In room temperature, air atmosphere, aluminium oxide ceramic substrate is placed in to coarsening solution, supersound process 20 minutes, adopt deionized water rinsing afterwards, obtains pretreated substrate.
The aqueous solution that described coarsening solution is hydrofluoric acid and Neutral ammonium fluoride, in coarsening solution, hydrofluoric acid concentration is 20ml/L, Neutral ammonium fluoride concentration 1g/L.
2, a nickel plating
To insert in the plating solution I through pretreated alumina-ceramic sample, after being 11 with sodium hydroxide adjusting pH, ultrasonic deposition 60 minutes, the ultrasonic frequency of ultrasonic deposition is 40KHz, and power is 300W, has reacted rear taking-up sample, use deionized water rinsing, and, in 80 ℃ of oven dryings 2 hours, room temperature is cooling, obtains the nickel plating substrate.
The aqueous solution that described plating solution I is single nickel salt, inferior sodium phosphate, boric acid and Trisodium Citrate, wherein the concentration of single nickel salt is 30g/L, and the ortho phosphorous acid na concn is 27g/L, and the concentration of boric acid is 30g/L, and the concentration of Trisodium Citrate is 60g/L.
3, secondary copper facing
The nickel plating substrate is put into to the plating solution II, and regulating pH with sodium hydroxide is 12,80 ℃ of heating in water bath for reaction 40 minutes, is cooled to room temperature with liquid afterwards, by deionized water rinsing drying, obtains the copper facing substrate.
The aqueous solution that described plating solution II is copper sulfate, formaldehyde, disodium ethylene diamine tetraacetate and 2,2-dipyridyl, wherein the concentration of copper sulfate is 13g/L, the concentration of formaldehyde is 25mL/L, the concentration of disodium ethylene diamine tetraacetate is 45g/L, and the concentration of 2,2-dipyridyl is 0.05g/L.
Alumina-ceramic surface metal copper layer prepared by the present embodiment, the film base is in conjunction with good, and coating compactness is good, and structural constituent is even.
Claims (6)
1. the method for an aluminium oxide ceramic substrate surface metalation, comprise alligatoring pre-treatment, a nickel plating and each unit process of secondary copper facing, it is characterized in that:
Described alligatoring pre-treatment is that aluminium oxide ceramic substrate is put into to coarsening solution supersound process 20-40 minute, uses afterwards deionized water rinsing, obtains pretreated substrate;
A described nickel plating is that described pretreated substrate is placed in to the plating solution I, and ultrasonic deposition 40-60 minute under room temperature uses deionized water rinsing after taking out, and obtains the nickel plating substrate after drying;
Described secondary copper facing is that described nickel plating substrate is placed in to the plating solution II, and in 60-80 ℃ of reaction 40-60 minute, cooling rear taking-up deionized water rinsing, obtain the copper facing substrate after drying.
2. the method for aluminium oxide ceramic substrate surface metalation according to claim 1 is characterized in that:
The aqueous solution that described coarsening solution is hydrofluoric acid and Neutral ammonium fluoride, in described coarsening solution, the concentration of hydrofluoric acid is 20-60ml/L, the concentration of Neutral ammonium fluoride is 1-4g/L;
Described plating solution I is the aqueous solution of single nickel salt, inferior sodium phosphate, boric acid and Trisodium Citrate, in described plating solution I, the concentration of single nickel salt is 20-30g/L, the ortho phosphorous acid na concn is 22-27g/L, and the concentration of boric acid is 24-30g/L, and the concentration of Trisodium Citrate is 50-60g/L.
3. the method for aluminium oxide ceramic substrate surface metalation according to claim 1 and 2 is characterized in that:
The pH value of described plating solution I is adjusted to 10-11 with sodium hydroxide.
4. the method for aluminium oxide ceramic substrate surface metalation according to claim 1 is characterized in that:
Described plating solution II is copper sulfate, formaldehyde, disodium ethylene diamine tetraacetate and 2, the aqueous solution of 2-dipyridyl, in described plating solution II, the concentration of copper sulfate is 10-13g/L, 2, the concentration of 2-dipyridyl is 0.03-0.05g/L, the concentration of formaldehyde is 15-25mL/L, and the concentration of disodium ethylene diamine tetraacetate is 35-45g/L.
5. according to the method for the described aluminium oxide ceramic substrate surface metalation of claim 1 or 4, it is characterized in that:
The pH value of described plating solution II is adjusted to 11-12 with sodium hydroxide.
6. the method for aluminium oxide ceramic substrate surface metalation according to claim 1 is characterized in that:
Ultrasonic frequency during described ultrasonic deposition is 40KHz, and power is 300-400W.
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| CN103928409A (en) * | 2014-03-17 | 2014-07-16 | 江苏省宜兴电子器件总厂 | Integrated circuit inverting welding air impermeability packaging structure |
| CN104048122A (en) * | 2013-08-02 | 2014-09-17 | 太仓派欧技术咨询服务有限公司 | SiC ceramic matrix composite nickel flange and preparation method thereof |
| CN105801179A (en) * | 2015-04-30 | 2016-07-27 | 深圳市环基实业有限公司 | Direct metallization method for ceramic substrate |
| CN107663108A (en) * | 2016-07-29 | 2018-02-06 | 比亚迪股份有限公司 | Ceramic coarsening solution and preparation method thereof and ceramic method of roughening |
| CN108385090A (en) * | 2018-02-27 | 2018-08-10 | 北京交通大学 | A kind of Ti of core/shell structure3C2Alkene/Cu powders and preparation method thereof |
| CN108440023A (en) * | 2018-04-20 | 2018-08-24 | 湖南省美程陶瓷科技有限公司 | A kind of method of aluminium oxide ceramics metallization |
| CN108531895A (en) * | 2018-03-29 | 2018-09-14 | 西安理工大学 | A method of the electroless deposition copper on aluminum oxide film |
| CN108569895A (en) * | 2018-04-20 | 2018-09-25 | 湖南省美程陶瓷科技有限公司 | A kind of preparation method of New-energy electric vehicle aluminium oxide ceramics |
| CN110467863A (en) * | 2019-08-16 | 2019-11-19 | 广东华祐新材料有限公司 | Conductive coating, plating solution, PCB circuit board and PCB circuit board production method |
| CN110729173A (en) * | 2019-09-23 | 2020-01-24 | 西安空间无线电技术研究所 | Method for improving adhesion of metal film layer of high-dielectric-constant ceramic substrate |
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| CN104048122A (en) * | 2013-08-02 | 2014-09-17 | 太仓派欧技术咨询服务有限公司 | SiC ceramic matrix composite nickel flange and preparation method thereof |
| CN103928409A (en) * | 2014-03-17 | 2014-07-16 | 江苏省宜兴电子器件总厂 | Integrated circuit inverting welding air impermeability packaging structure |
| CN103928409B (en) * | 2014-03-17 | 2017-01-04 | 江苏省宜兴电子器件总厂 | A kind of integrated circuit back-off weldering air-tight packaging structure |
| CN105801179A (en) * | 2015-04-30 | 2016-07-27 | 深圳市环基实业有限公司 | Direct metallization method for ceramic substrate |
| CN105801179B (en) * | 2015-04-30 | 2018-03-16 | 深圳市环基实业有限公司 | A kind of ceramic substrate substrate surfaces method |
| CN107663108A (en) * | 2016-07-29 | 2018-02-06 | 比亚迪股份有限公司 | Ceramic coarsening solution and preparation method thereof and ceramic method of roughening |
| CN108385090A (en) * | 2018-02-27 | 2018-08-10 | 北京交通大学 | A kind of Ti of core/shell structure3C2Alkene/Cu powders and preparation method thereof |
| CN108385090B (en) * | 2018-02-27 | 2020-05-08 | 北京交通大学 | Core/shell structure Ti3C2alkene/Cu powder and preparation method thereof |
| CN108531895A (en) * | 2018-03-29 | 2018-09-14 | 西安理工大学 | A method of the electroless deposition copper on aluminum oxide film |
| CN108440023A (en) * | 2018-04-20 | 2018-08-24 | 湖南省美程陶瓷科技有限公司 | A kind of method of aluminium oxide ceramics metallization |
| CN108569895A (en) * | 2018-04-20 | 2018-09-25 | 湖南省美程陶瓷科技有限公司 | A kind of preparation method of New-energy electric vehicle aluminium oxide ceramics |
| CN110467863A (en) * | 2019-08-16 | 2019-11-19 | 广东华祐新材料有限公司 | Conductive coating, plating solution, PCB circuit board and PCB circuit board production method |
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